钛粉含量和零氧平衡协同下CO<sub>2</sub>相变激发药剂的性能表征

杜明燃; 李韦伟; 王尹军; 杨海斌; 李继红

doi:10.11858/gywlxb.20240866

钛粉含量和零氧平衡协同下CO₂相变激发药剂的性能表征

doi: 10.11858/gywlxb.20240866

1.
安徽理工大学化工与爆破学院, 安徽淮南　232001
2.
矿冶科技集团有限公司, 北京　100160
3.
中国矿业大学(北京)力学与建筑工程学院, 北京　100083
4.
河北云山化工集团有限公司, 河北邢台　054011

基金项目: 安徽高校自然科学研究项目（KJ2021A0431）；安徽省自然科学基金（1908085QA33）；安徽理工大学引进人才基金（11881）

详细信息

作者简介:
杜明燃（1987－），男，博士，副教授，主要从事炸药性能和爆破技术研究. E-mail：466199112@qq.com

中图分类号: TJ510.4; O389; O521.2
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出版历程
- 收稿日期: 2024-08-06
- 修回日期: 2024-08-19
- 刊出日期: 2025-03-05

Performance Characterization of CO₂ Phase Change Excitation Agent under the Synergistic Effect of Titanium Powder Content and Zero Oxygen Balance

1.
School of Chemical and Blasting Engineering, Anhui University of Science and Technology, Huainan 232001, Anhui, China
2.
BGRIMM Technology Group, Beijing 100160, China
3.
School of Mechanics & Civil Engineering, China University of Mining & Technology, Beijing 100083, China
4.
Hebei Yunshan Chemical Group Co., Ltd., Xingtai 054011, Hebei, China

摘要

摘要: 为了提高CO₂相变激发药剂的性能，向激发药剂中分别加入质量分数为2%、4%、6%、8%和10%的钛粉，并调整草酸铵和水杨酸含量，使药剂接近零氧平衡，通过现场引燃试验、热重法、耐温性能测试和理论计算，研究其引燃可靠性、压力性能、热分解特性、安全性能和耐温性能。结果表明：加入质量分数为2%、4%、6%、8%的钛粉后，管内激发药剂均能被成功引燃；峰值压力与药剂放热量直接相关，在本试验的添加范围内，质量分数为8%钛粉激发药剂的管内压力性能最好；添加8%钛粉不调整零氧平衡、通过草酸铵调整零氧平衡、通过水杨酸调整零氧平衡的峰值压力分别提高了11.81%、14.27%、17.85%；3个样品的表观活化能变化分别为−5.96、33.47 和6.80 kJ/mol；调整零氧平衡可以优化激发药剂的热稳定性，加入8%钛粉后激发药剂的安全性良好，温度指数T_s均在90 ℃以上。
- 二氧化碳相变爆炸 /
- 激发药剂 /
- 零氧平衡 /
- 钛粉含量
Abstract: To improve the performance of the CO₂ phase change excitation agent, titanium powder with mass fractions of 2%, 4%, 6%, 8%, and 10% was added to the excitation agent. The contents of ammonium oxalate and salicylic acid were controlled to adjust the zero oxygen balance, respectively. The ignition reliability, pressure performance, thermal decomposition characteristics, safety performance and temperature resistance property were investigated by on-site ignition tests, thermogravimetric analysis, temperature resistance performance tests and theoretical calculations. The results show that: all the excitation agents are successfully ignited inside the tube after adding titanium powder with mass fractions of 2%, 4%, 6%, and 8%. The peak pressure is directly associated with the heat release amount of the excitation agent. Within the addition range of this test, the excitation agent with 8% titanium powder has the best pressure performance inside the tube. After adding titanium powder with a mass fraction of 8%, the peak pressures of excitation agent without adjusting the oxygen balance, with adjusting the zero oxygen balance through ammonium oxalate, and with adjusting the zero oxygen balance through salicylic acid increase by 11.81%, 14.27%, and 17.85%, respectively. The apparent activation energies of the three samples decrease by 5.96 kJ/mol, increase by 33.47 and 6.80 kJ/mol, respectively, indicating that adjusting the zero oxygen balance can optimize the thermal stability of the excitation agent. After adding titanium powder with a mass fraction of 8%, the safety of the excitation agent is good, and the temperature index T_s is above 90 ℃.
- CO₂ phase change explosion /
- excitation agent /
- zero oxygen balance /
- titanium powder content

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图 1 引燃药包样品

Figure 1. Ignition drug pack samples

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图 2 液态CO₂充装示意图

Figure 2. Schematic diagram of liquid CO₂ filling

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图 3 部分药包引燃后的状态

Figure 3. Post-ignition status of partial drug packets

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图 4 露天引燃试验结果

Figure 4. Results of the outdoor ignition tests

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图 5 管内引燃试验结果

Figure 5. Ignition test results inside the tube

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图 6 致裂管中各组样品测点处的压力波形

Figure 6. Pressure waveform at the measuring point of each group of samples in the cracking tube

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图 7 不同样品的峰值压力

Figure 7. Peak pressure of different samples

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图 8 不同样品的反应热理论值与峰值压力的关系

Figure 8. Relationships between theoretical values of reaction heat and peak pressure of different samples

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图 9 液态CO₂充装量与峰值压力的关系

Figure 9. Relationships between liquid CO₂ filling quantity and peak pressure

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图 10 激发药剂的TG曲线

Figure 10. TG curves of excitation agent

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图 11 激发药剂的DTG曲线

Figure 11. DTG curves of excitation agent

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图 12 采用Ozawa法得到的lg β-10³/T曲线拟合结果

Figure 12. Fitting results of lg β-10³/T by Ozawa’s method

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图 13 常温储存下不同激发药剂样品的XRD谱

Figure 13. XRD profiles of different excitation agent samples after storage at room temperature

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图 14 部分样品干燥前、后的状态

Figure 14. State of partial samples before and after drying

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表 1 基础激发药剂样品的配比

Table 1. Basic excitation agent sample formula

Sample	Mass/g				ω_Ti/%	OB/（g·g⁻¹）
Sample	KClO₄	C₂H₈N₂O₄	C₇H₆O₃	Ti	ω_Ti/%	OB/（g·g⁻¹）
1	82.439	35.366	12.195	0	0	0.00035
2	82.439	35.366	12.195	2.6	1.96	−0.01272
3	82.439	35.366	12.195	5.2	3.85	−0.02530
4	82.439	35.366	12.195	7.8	5.66	−0.03740
5	82.439	35.366	12.195	10.4	7.40	−0.04905
6	82.439	35.366	12.195	13.0	9.09	−0.06028

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表 2 草酸铵调整零氧平衡样品的配比

Table 2. Sample formula of adjusting zero oxygen balance by the content of ammonium oxalate

Sample	Mass/g				ω_Ti/%	OB/（g·g⁻¹）
Sample	KClO₄	C₂H₈N₂O₄	C₇H₆O₃	Ti	ω_Ti/%	OB/（g·g⁻¹）
7	82.439	32.076	12.195	2.6	2.01	0.00001
8	82.439	28.712	12.195	5.2	4.05	0.00001
9	82.439	25.352	12.195	7.8	6.10	0.00001
10	82.439	22.005	12.195	10.4	8.19	0.00001
11	82.439	18.661	12.195	13.0	10.29	0.00001

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表 3 水杨酸调整零氧平衡样品的配比

Table 3. Sample formula of adjusting zero oxygen balance by the content of salicylic acid

Sample	Mass/g				ω_Ti/%	OB/（g·g⁻¹）
Sample	KClO₄	C₂H₈N₂O₄	C₇H₆O₃	Ti	ω_Ti/%	OB/（g·g⁻¹）
12	82.439	35.366	11.146	2.6	1.97	0.00001
13	82.439	35.366	10.036	5.2	3.90	0.00001
14	82.439	35.366	9.013	7.8	5.78	0.00001
15	82.439	35.366	7.952	10.4	7.62	0.00001
16	82.439	35.366	6.894	13.0	9.44	0.00001

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表 4 试验样品的峰值压力数据

Table 4. Peak pressure data of the test samples

Group	Sample	Empty tube quality/kg	Tube quality after filling liquid/kg	Liquid CO₂ charge amount/g	Surge pressure/MPa
1	1	13.856	14.709	853	157.1
	2	13.855	14.683	828	162.1
	3	13.854	14.727	873	167.5
	4	13.856	14.679	823	168.9
	5	13.856	14.698	842	179.5
	7	13.855	14.719	864	162.4
	8	13.854	14.691	837	168.6
	9	13.858	14.700	842	169.9
	10	13.856	14.731	875	179.8
	12	13.854	14.721	867	166.3
	13	13.855	14.727	872	170.5
	14	13.855	14.718	833	177.3
	15	13.855	14.737	882	183.2
2	1	13.858	14.699	841	158.2
	2	13.856	14.723	867	163.4
	3	13.855	14.711	856	166.9
	4	13.857	14.699	842	169.5
	5	13.854	14.740	886	172.4
	7	13.856	14.710	854	163.3
	8	13.855	14.718	863	169.2
	9	13.856	14.712	856	172.5
	10	13.855	14.686	831	180.5
	12	13.857	14.711	854	164.8
	13	13.856	14.702	846	174.6
	14	13.856	14.695	869	178.1
	15	13.854	14.705	851	186.5

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表 5 激发药剂反应热理论值

Table 5. Theoretical reaction heat values of excitation agent

Sample	ΔH_T/（kJ·kg⁻¹）
1	5203.0
2	5261.5
3	5311.8
4	5360.1
5	5406.7
7	5325.7
8	5447.3
9	5570.4
10	5694.3
12	5363.3
13	5516.7
14	5668.2
15	5816.2

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表 6 各样品的瞬间压剪速度

Table 6. Instantaneous compression-shear speed of each sample

Sample	Pressure rise time/ms		Instantaneous compression-shear speed/（m·s⁻¹）		Average instantaneous compression-shear speed/（m·s⁻¹）
Sample	Group 1	Group 2	Group 1	Group 2	Average instantaneous compression-shear speed/（m·s⁻¹）
1	2.82	5.86	156.03	75.09	115.56
2	3.03	1.72	145.21	255.81	200.51
3	2.61	2.58	168.58	170.54	169.56
4	1.26	3.21	349.21	137.07	243.14
5	4.04	2.92	108.91	150.68	129.80
7	3.06	4.22	143.79	104.27	124.03
8	2.53	2.54	173.91	173.23	173.57
9	4.69	2.11	93.82	208.53	151.17
10	1.54	3.68	285.71	119.57	202.64
12	2.54	5.02	173.23	87.65	130.44
13	3.69	4.29	119.24	102.56	110.90
14	3.66	1.82	120.22	241.76	180.99
15	2.74	1.61	160.58	273.29	216.94

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表 7 Ozawa法计算各样品的动力学参数

Table 7. Kinetic parameters of each sample obtained by Ozawa’ method

$ \alpha $/%	E/（kJ·mol⁻¹）				r²
$ \alpha $/%	Sample 1	Sample 5	Sample 10	Sample 15	Sample 1	Sample 5	Sample 10	Sample 15
5	69.89	70.26	81.52	71.08	0.9933	0.9721	0.9993	0.9871
10	71.84	81.79	113.43	89.70	0.9993	0.9933	0.9993	0.9746
15	183.65	171.82	216.36	190.80	0.9715	0.9972	0.9861	0.9919
20	171.30	167.41	210.54	181.99	0.9890	0.9852	0.9942	0.9860
25	194.08	188.72	206.92	184.03	0.9815	0.9859	0.9926	0.9852
30	120.16	95.16	182.96	134.09	0.9998	0.9746	0.9509	0.9763
Average value	135.15	129.19	168.62	141.95

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表 8 各样品干燥前、后的质量

Table 8. Mass of each sample before and after drying

Sample	Mass/g		Hot weightlessness/%
Sample	Before drying	After drying	Hot weightlessness/%
1	10.00	7.83	21.7
2	10.00	7.98	20.2
3	10.00	7.93	20.7
4	10.00	7.95	20.5
5	10.00	8.01	19.9
7	10.00	8.22	17.8
8	10.00	8.32	16.8
9	10.00	8.47	15.3
10	10.00	8.42	15.8
12	10.00	7.86	21.4
13	10.00	7.85	21.5
14	10.00	7.91	20.9
15	10.00	7.90	21.0

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